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Visible light-driven photocatalysts based on TiO 2 have significant potential for providing sustainable fuel for the future. Layered titanates, which have unique structures, are a focus of considerable research attention due to their ease of interconversion into new nanoarchitectures of TiO 2 that have high photocatalytic performance. We describe here the synthesis of CuO nanostructures from the interconversion of copper titanate during the generation of TiO 2 nanosheets. We further examined the in situ structural transformation of the CuO-loaded TiO 2 nanosheets during photocatalytic hydrogen production from ammonia−borane (NH 3 •BH 3 ; AB) under visible light and studied the impact of the reaction media and of photoirradiation on the catalyst's final structure by characterizing the recovered catalyst using X-ray diffraction (XRD), UV−vis, and transmission electron microscopy (TEM) analyses. The results show that the CuO nanoparticles are converted to metallic Cu nanoparticles, which photocatalyze the reaction through their in situ-formed plasmonic features. The potential role of the introduced plasmonic Cu nanoparticles in promoting charge separation and enhancing photocatalytic performance is also investigated.

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